Hydroxyamine hydrochloride → HCID 178526312, compound

Participants

Reaction Steps

A mixture of 3-phenylindeno[1,2-c]pyrazol-4(1H)-one (1.28 g, prepared as described in JP60-130521), hydroxylamine hydrochloride (0.5 g), sodium acetate (0.8 g), water (10 ml) and methanol (100 ml) was boiled under reflux for 66 hours. More hydroxylamine hydrochloride (0.5 g), sodium acetate (0.8 g) and water (10 ml) were added and the mixture was boiled under reflux for a further 16 hours. Further hydroxylamine hydrochloride (0.5 g) and sodium acetate (0.8 g) were added and the mixture was boiled under reflux for a further 20 hours. The mixture was filtered and the filtrate was concentrated under reduced pressure until crystallization began. The mixture was cooled and filtered to give a solid which was washed with water and dried to give 3-phenylindeno[1,2-c]pyrazol-4(1H)-one oxime, m.p. 280° C. (with decomposition).

Provenance & Evidence